yields

[geezmeister]

Never ever add I2 to a mixture of H2O+P+E ! This will ruin your yields.

Odd. This has not been my experience at all.

And another thing to note here is to do freebase rxns

Freebase reactions do seem to give some advantage. There was a debate in this forum over yields from freebase reactions as opposed to reactions done with the HCl form. For a long time, I was convinced that the freebase form was the reason for the generally better yields from freebase reactions. At one particular time one of the extraction techniques I employed was particularly successful at producing very very clean HCl form pseudo...after two recrystallizations in alcohol and acetone, I would have brad like spikes of pseudo to react... To my amazement, the best yields I obtained were from reactions of that pseudo HCl. Granted, the difference between my best HCl yeild and my best freebase yield was was less than a percentage point. The experience convinced me that HCl was not deleterious to the reaction...and that the higher yields I had experienced from the freebase form was in fact due to it being cleaner on the whole than the salt form. Every time I cleaned pseudo HCl until the recrystallization in alcohol made those spikes, I got the same results. 

Then the mix should be gently refluxed in an oilbath at 160c for at LEAST 48 hours.

Experience in this area indicated to me that an in-flask temperature of 100c was sufficient, and it was unnecessary to exceed an in flask temperature of 120C. We may be discussing the same temperature, if you are using the temperature of the oil bath. I also found that forty eight hour reactions on the whole gave a superior product to 36 hour reactions, but the edge was very small. There is a large difference in quality between eight hours and twenty four; less between twenty four and thirty six; and even less between thirty six and forty eight.

[SHORTY]

Odd. This has not been my experience at all.

Nor have i experienced any noticeable yield loss from doing this.

Hopefully, the 160C is the temp of the oil since 57% HI has a bp of 126C.  Even so that would be a 34 degree difference between the internal flask and the oil.  Last time i checked the difference in my setup is around 15C or less but it depends on the setup.

[lutesium]

Speaking generally

SWIM never tested his statements of adding I2 to P+H2O+E mixture and its effects on the yield but he knows for sure that a reaction should be controlled as much as possible and sudden temprature peaks are dangerous for any type of reaction. And I2 reacts very exhothermically with P and the resultant PI3 is also very reactive so why ask for trouble when you can first let the exhothermic storm pass then add whatever you want to be reduced in?

Of course refluxing for 48 hours can be substituted for less but a chemist wants to be sure the rxn gives maximum yields possible so he should give it enough time to complete as more doesn't hurt. And SWIM believes that this is a kind of complicated reaction which has a VERY complicated mechanism. So enough time seems like the only guarantee that may save a incomplete reduction.

And 160c is the temprature of the bath. Remember that SWIM suggested a very large excess of HI and with these ratios the reaction should gently reflux at this temprature

[pillboy37]

Swim is not trying to be a smart ass here,but how about letting the rest of the world know your secret.
  Their hasn,t been a latest method that has been posted here or any where else for that matter that will produce a clean 80% yield of goddies from OTC stock in a while,and thats using Lab Gr.I,and decent quality red.
 Like swim said,not trying to be an ass,just wanting to know if he's missed something.

[Calibron]

"Swim is not trying to be a smart ass here,but how about letting the rest of the world know your secret."

You see, that is the problem with keeping secrets, if we were to let the whole world know, then it wouldn't bee a secret anymore now would it? Truth bee told, it is not a secret! It is already in the search engine and any repetition should bee rated as "Redundant"  

Everytime they PUSH the new extraction methods, "THEY" add new gakk or surfactants and then WE as a collective are back to square one, trying to find a new cure. Fuck that! If bees want to succeed they will learn to use the search function and computer skills. No more handouts or spoon feeding!

Pills are now readily available to the clandestinely motivated, not just any highschool tweeker that shows up at the site, reads 3 threads, spreads it around by loose lips to anyone who cares to listen (including LE) and in the process, destroys highly valued availability. Most of whom cater to the mexican cartels when the chips are down anyway.

I suppose the priviledged should sacrifice their sources and open their wallets to YOU as well? It is NOT a secret, it is in TFSE... USE IT!

Spoon feeding is an insult to those of US, who spend hours every day reading threads and using the search engine, (religiously) working overtime via DO BEE experiments with OTC solvents to help develop these cures that theoretically, barely pay the bills and only serve to make pharmaceutical companies richer.  

The fewer pills that these fuckers are able to sell, the less likely that they are to step UP their efforts to further prevent extraction.  

[pillboy37]

It,s not a matter of finding it on the search engine.The point is ,its not there to find.
 The days are long gone,at least in this area, of even getting close to an 80% return using a RP/I reduction on OTC stock. It,s not going to happen.
 You can say what you want,but swim ain,t never took the easy way out and read "3 or 4 post" and tried to make it work.
 Hell, if you,ll notice ,swim was logged on to this site for allmost a year befor swim ever asked for any help,and that year was spent reading and reading and reading.
 No, swim ain't asking for nothing, just saying in this part of the states with an RP/I reduction you AINT going to pull 80% dont care what extraction method you use.
 Not scince the STE first came out have those #,s even been close to 80%.

[abominator]

I can understand what you are saying pillboy, but there are methods within the hive that will yeild clean enough feedstock, plus you can polish it UP with a few different methods.  i.e. pfed precip...  ...# of rextals...  There are also many bees who reguraly report of 80% yields.

As far as pillstock cleaning methods, Fester's hydrolosis works, BarkingBurrows method works and so does Evilscripter69's(cool username btw ).  Just give them a whirl and swim don't see why you can't get back 80%, he did on his last reflax.

[CharlieBigpotato]

what beecomes of the chlorine in the rdxn of psuedo-hcl, anyway?
i can't seem to locate it.

[wareami]

In the few 49 or so posts I've been priveleged enough to read, lutesium speaks good medicine and is reminiscient of an incarnation of an elderbee seldom seen these days!
I could be wrong!
None-the-less...I concur with the idealogy and advice coming from that corner.
However minute, the "generally speaking" advice about exothermicity and yields/full reduction is the advice that helped to form Ibee's early experimentation with the less violent LWR rxn.
Slow Controlled is far better AWE the way around with the HI/RP rxn IMHO.

CBP:You don't reckon that the chlorine smell Ibee smells when steam distilling is that -CL molecule do ya?
Could bee!
Never really thought about it til now!

[CharlieBigpotato]

wareami;
don't know, but i'd suspect the Cl must bond to something in the stew beefore we dump it from a dream.
same w/ P

[Rhodium]

what beecomes of the chlorine in the rdxn of psuedo-hcl, anyway? i can't seem to locate it.

The HCl turns into NaCl in the post-rxn basification and stays in the aqueous phase during workup. It never gets oxidized to free chlorine gas.

[Jacked]

SPINNERBAIT, Swim has been running this shit for quite some time now and 70% is as high as he would ever expect. That was using E from china. E strait from the manufacture. Swim also experienced 70% returns using pill stock from the US, The trouble was in getting a good yield from the pill itself. Kerplunking is a good yield point for RP/I2 post reaction workups and the advice given about driving the pH down a little bit more is also good advice.. Don't be afraid of using to much H2O when titrating. In other words "don't sweat the evap until its time to evap". People using little bits of H20 worried about evap times wind up pulling more than twice, and before there done they have about the same amount of water anyway usually with more salt from the third pull added and just took more time getting it. Also give the Ph time to stabilize before separating the H2O from the non polar..
 With todays pill problems yield suffers right off the bat before the reaction takes place. Refine your process and only change one thing at a time, record your findings so you can compare notes to changes made, once you increase your yield by making a change try to repeat it. Keep working at it and always tweak your process. In time you will be spouting off high yields and be answering other peoples questions about yields..
 I'm surprised at the response you have gotten from the limited amount of information you gave. That in it self is rare it must be a good day at the hive. The more information you give the better information you will receive is generally the rule..
Most Important and read carefully.
 As far as bees that keep secrets from bees but tantalize you with there experience. Don't place your faith in that information. You should always give more than you take from your beloved hive. At first you will only take because you wont have much to give, in time its only right to give back to the place that gave you so much. After all if everyone practiced secretly there would be only boasting and flaming and no chemistry at all here. This is not how the hive works. Always respect the time and effort bees take to help you along in this craft. If you don't choose to input because of one thing or another then you can always donate some cash to help in the up keep around here

[geezmeister]

Well said, Jacked. I hope every new bee reads your post two or three times and gives some thought about the advice you give.

It is great advice. It pays excellent dividends.

[wareami]

Deserves the World's Largest Smiley in my book!
"If you smile at me i will understand, because that is something
everyone everywhere does in the same language"
- crosby, stills and nash -